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2,3,4,5-Tetrahydro-1-benzoxepin-5-one → 3,4-dihydro-1-benzoxepin-5(2H)-one oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,3,4,5-Tetrahydro-1-benzoxepin-5-one | HCID 315575 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 3,4-dihydro-1-benzoxepin-5(2H)-one oxime | HCID 73200353 | 92.8% |
反応手順
A solution of 10.0 g (62 mmol) of 3,4-dihydro-1-benzoxepin-5(2H)-one (J. Chem. Soc., Perkin Trans. 1 (1991), 2763) and 4.63 g (68 mmol) of hydroxylamine hydrochloride in 45 ml of ethanol and 45 ml of pyridine was heated under reflux for 5 h. After distilling off the solvents on a rotary evaporator, the residue was treated with water, adjusted to pH 2 with dil. hydrochloric acid and stirred for 3 h. After filtering off the precipitated product with suction and drying it, 10.2 g of 3,4-dihydro-1-benzoxepin-5(2H)-one oxime were obtained, m.p. 96-98° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06333349B1 |
| 出典データセット | uspto-grants-2001_12 |
| ORD ID | ord-088a30e1f5564441806dd06c265ab31f |
| 出典メモ | uspto-grants-2001_12 |